烯酰吗啉合成新工艺研究

Study on a new synthesis process of enoylmorpholine

为降低烯酰吗啉合成过程中N-乙酰吗啉的消耗,降低生产成本,在反应过程中加入了缚碱剂,以减少N-乙酰吗啉的分解。以4-氯-3',4'-二甲氧基二苯甲酮(E-苯酮)和N-乙酰吗啉为原料,二甲苯为溶剂,N,N-二甲基甲酰胺为缚碱剂,在叔丁醇钠催化作用下合成了烯酰吗啉。考察了投料比、反应温度、反应时间等因素对合成的影响,优化的反应条件为n(E-苯酮)∶n(N-乙酰吗啉)∶n(叔丁醇钠)∶n(N,N-二甲基甲酰胺)=1.00∶1.05∶1.15∶1.25,反应温度为135℃,反应时间为10 h,在此条件下产品烯酰吗啉收率90.8%,纯度97.6%。

To reduce the consumption of N-acetylmorpholine in the synthesis process of enoylmorpholine and lower production costs,a base binding agent was added during the reaction to reduce the decomposition of N-acetylmorpholine.Enoylmorpholine was synthesized using 4-chloro-3',4'-dimethoxybenzophenone(E-phenyl ketone)and N-acetylmorpholine as raw materials,xylene as solvent,and N,N-dimethylformamide as a base binding agent under the catalysis of sodium tert butanol.The influence of factors such as feed ratio,reaction temperature,and reaction time on the synthesis was investigated.The optimized reaction conditions were as follows,n(E-phenyl ketone)∶n(N-acetylmorpholine)∶n(sodium tert butanol)∶n(N,N-dimethylformamide)=1.00∶1.05∶1.15∶1.25,reaction temperature was 135℃,and reaction time was 10 hours.Under these conditions,the yield of the product enoylmorpholine was 90.8%,and the purity was 97.6%.